Micro-area variable angle grazing incidence wide-angle scattering test method

Abstract

The present invention proposes a micro-area variable angle grazing incidence wide-angle scattering test method based on a single crystal X-ray diffractometer, including preparing a sample of a test material deposited on a substrate and placing it on an improved sample holder, the improved sample holder having a specific structure and a driver for controlling the incident angle, etc.; selecting an X-ray light source and aligning it with the sample, using a copper target and a molybdenum target for switching and matching; performing a Z-scan scan and a tilt scan along the optical path direction and perpendicular to the optical path direction, and setting relevant parameters; collecting the scattered X-rays through a two-dimensional surface detector; and finally obtaining a related graph through software integration. The table size, scanning parameters, etc. of the improved sample holder have specific requirements, and a height reference position, an adjustment structure, etc. are also provided, and the connection part is installed on the equipment sample table by screwing. The present invention solves the problems of inaccurate control of the incident angle and height in the prior art, and improves the accuracy and reliability of the test.

Description

Technical Field

[0001] The invention relates to the interdisciplinary field of material science and physics, and in particular to a micro-area variable-angle grazing-incidence wide-angle scattering test method based on an X-ray single crystal diffractometer. Background Art

[0002] At present, wide-angle scattering test methods and devices based on small-angle X-ray scattering instruments are commonly used materials analysis tools, and wide-angle scattering test methods based on single crystal XRD (single crystal diffractometer) are also gradually being developed and promoted. However, this device faces many problems in grazing incidence wide-angle scattering tests. The defects of existing devices are:

[0003] (1) Incident angle control problem

[0004] In the process of grazing incidence wide-angle scattering, the existing device cannot accurately control the incident angle and cannot realize micro-area variable angle grazing incidence wide-angle scattering test. Testers often place samples based on their own experience and feel, which cannot guarantee the flatness of the sample surface horizontally along the light path and horizontally perpendicular to the light path. Insufficient flatness is bound to affect the test results, such as causing interference with the scattering intensity and failing to accurately obtain relevant characteristic information of the material.

[0005] (2) Altitude control issues

[0006] The grazing incidence wide-angle scattering in this environment cannot be precisely controlled in terms of height. Imprecise height control not only affects the scattering intensity, but also causes the drift of the diffraction peaks in the scattering spectrum and severe scattering background. The drift of the diffraction peaks makes the analysis of the test data in the future ambiguous, which seriously affects the accuracy and reliability of the test results, and thus limits the further application and development of this technology in the field of material analysis.

[0007] In summary, the existing wide-angle scattering test technology based on single crystal XRD has shortcomings in the control of incident angle and height. A new technical solution is urgently needed to solve these problems in order to improve the accuracy, reproducibility and reliability of the test and expand its application scope in the field of material analysis. Summary of the invention

[0008] The embodiment of the present invention provides a micro-area variable angle grazing incidence wide-angle scattering test method, which aims to solve the problems of inaccurate control of the incident angle and height of grazing incidence wide-angle scattering in the current technology, which affects the scattering intensity and causes the diffraction peak position drift, as well as insufficient sample surface flatness.

[0009] The core technology of the present invention is mainly based on a quaternary single crystal diffractometer. By improving the design of the sample holder and specific test steps and parameter settings, including precise control of the incident angle, height, etc., accurate testing of micro-area variable-angle grazing-incidence wide-angle scattering is achieved, solving the defects of the prior art in this field.

[0010] In a first aspect, the present invention provides a micro-area variable angle grazing incidence wide-angle scattering test method, the method comprising the following steps:

[0011] S00, preparing a sample of the test material deposited on the substrate and placing it on an improved sample holder;

[0012] The improved sample holder is used to replace the original sample holder of the single crystal diffractometer, and the improved sample holder is provided with a table for placing test materials, a Z-axis height reference position, a height adjustment driver for driving the improved sample holder to move back and forth along the Z-axis, an arc adjustment driver for driving the improved sample holder to perform a curved swinging motion along the optical path direction, and a connection part that cooperates with the sample stage of the single crystal diffractometer, and the control of the incident angle is realized by the arc adjustment driver;

[0013] S10, selecting an X-ray light source, aligning the X-ray light source at the sample, and switching between a copper target and a molybdenum target;

[0014] S20, in the Z-scan scanning mode of the single crystal diffractometer, performing X-ray light intensity scanning in the vertical direction, and adjusting the test material with the substrate to a test height through the lifting drive component of the single crystal diffractometer;

[0015] S30, performing a tilt scan along the optical path on the improved sample holder, scanning from the minimum light flux to the strongest light and then to the weakest light, taking the Theta angle when the light intensity is the strongest as the zero point of the optical path direction, and setting the distance between the sample and the detection surface of the single crystal diffractometer, the exposure time and the incident angle;

[0016] S40, collecting scattered X-rays through a two-dimensional surface detector;

[0017] S50, integrating by software of a single crystal diffractometer to obtain a one-dimensional X-ray scattering diagram;

[0018] The incident angle is continuously changed, and the scattered X-rays are continuously collected through a two-dimensional surface detector, and then integrated through software to obtain a series of one-dimensional X-ray scattering maps.

[0019] Furthermore, the planar size of the table top of the improved sample rack is less than or equal to 1 cm x 1 cm.

[0020] Furthermore, in step S20, the scanning parameters of the Z-scan scanning mode are: Z scanning range 0-20 mm, step length 0.1 mm / step, scanning speed 0.1 s / step.

[0021] Furthermore, in step S30, the distance between the sample and the detection surface of the single crystal diffractometer is 40-120 mm, the exposure time is 1-300 s, and the incident angle is 0.1-10°.

[0022] Furthermore, the Z-axis height reference position is taken as 0 mm.

[0023] Furthermore, the improved sample rack is also provided with an adjustment structure for adjusting the horizontal position of the table top.

[0024] Furthermore, the connection portion is screwed to install the improved sample holder on the sample stage of the single crystal diffractometer.

[0025] Furthermore, the adjustment structure includes an X-axis adjustment screw for adjusting the X-axis position of the table and a Y-axis adjustment screw for adjusting the Y-axis position of the table.

[0026] Furthermore, the connection portion is screwed to install the improved sample holder on the sample stage base of the single crystal diffractometer.

[0027] Furthermore, the sample holder is provided with an arc adjustment screw for adjusting the arc of the tabletop swing. The arc adjustment screw is arranged perpendicularly to the output shaft of the arc adjustment driver, and can adjust the substrate to a flat horizontal line to optimize the scattering intensity.

[0028] Furthermore, the curvature adjustment screw is also connected to a curvature adjustment driver.

[0029] The main contributions and innovations of the present invention are as follows:

[0030] 1. Improve test accuracy

[0031] Precise control of the incident angle: By improving the design of the sample holder, an arc adjustment driver is provided to drive the sample stage to make a curved swinging motion along the direction of the optical path, thereby achieving precise control of the incident angle of micro-area variable-angle grazing incidence scattering, avoiding the problem of inaccurate incident angle caused by placing samples based solely on experience and feel in the prior art, improving the parallelism and reproducibility of the test, and thus being able to more accurately obtain the scattering information of the material.

[0032] High-precision height control: The improved sample holder is equipped with a Z-axis height reference position, and digital high-precision height control is achieved through related components to ensure that the scattering spectra of all samples do not drift, ensure the standardization and reproducibility of the test peak position, improve data quality, and overcome the problems of scattering intensity affected and diffraction peak position drift caused by inaccurate height control in the existing technology.

[0033] 2. Expand the depth and scope of material analysis

[0034] Depth gradient profiling: Precisely controlled incident angles can expand the depth gradient profiling of thin film materials deposited on substrate materials based on the original technology, and achieve structural gradient changes from the surface to the bulk of the material. This can be applied to the analysis of a variety of materials such as solar cell materials, solid fuel cells, green energy catalysts, organic photovoltaics, and chips for data storage and transmission. Existing technologies are limited in this regard.

[0035] Micro-area analysis capability: By utilizing the 100-micron focal spot characteristic of the single crystal XRD light source, the improved sample holder can achieve high-precision micro-area analysis through relevant settings. The sample can be moved by fine-tuning X and Y to achieve micro-area variable-angle grazing-incidence wide-angle scattering characterization in different regions. Existing technologies cannot meet the needs of this micro-area analysis.

[0036] In-situ monitoring and analysis capabilities: The temperature control system can realize the construction of atmosphere purge and variable temperature in-situ environment, and realize micro-area variable angle grazing incidence wide-angle scattering monitoring under in-situ conditions, which greatly expands the analysis breadth of the hardware.

[0037] 3. Improve test safety and convenience

[0038] Protect component safety: The improved sample holder is flexible and compact, breaking through the limitation of the narrow space between the collimator and the light blocker. It can not only meet all the test requirements of micro-area variable-angle grazing incidence scattering, but also maximize the protection of the safety of components such as detectors. The existing technology is insufficient in this regard.

[0039] Systematic testing steps: The present invention designs a complete testing method, including various steps from sample preparation, light source selection, scanning mode to signal acquisition and processing, and the parameters of each step are clear, the operation is more standardized and convenient, and the test efficiency and reliability are improved. Compared with the inaccurate operation and lack of systematicity of the prior art, it has obvious advantages.

[0040] Low modification cost: The sample holder can be directly modified and replaced on the existing quaternary single crystal diffractometer without the need for complex structural improvements, and the modification cost is low.

[0041] The details of one or more embodiments of the invention are set forth in the following drawings and description so that other features, objects, and advantages of the invention are more readily apparent. BRIEF DESCRIPTION OF THE DRAWINGS

[0042] The drawings described herein are used to provide a further understanding of the present invention and constitute a part of the present invention. The exemplary embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an improper limitation of the present invention. In the drawings:

[0043] Figure 1 is a flow chart of a micro-area variable angle grazing incidence wide-angle scattering test method according to an embodiment of the present invention;

[0044] Figure 2 is a schematic diagram of the basic structure of a single crystal diffractometer according to an embodiment of the present invention;

[0045] Figure 3 is a scattering diagram obtained by a two-dimensional surface detector during a scanning process of a micro-area variable angle grazing incidence wide-angle scattering test method according to an embodiment of the present invention;

[0046] Figure 4 It is a two-dimensional scattering diagram obtained by adjusting parameters of a two-dimensional surface detector for the first time (using arc adjustment along the optical path direction) during a scanning process of a micro-area variable angle grazing incidence wide-angle scattering test method according to an embodiment of the present invention;

[0047] Figure 5 It is a two-dimensional scattering diagram obtained by a two-dimensional surface detector during the second parameter adjustment (using another arc adjustment) during the scanning process of the micro-area variable angle grazing incidence wide-angle scattering test method according to an embodiment of the present invention;

[0048] Figure 6 is a two-dimensional scattering diagram obtained by a two-dimensional surface detector after adjustment during a scanning process of a micro-area variable angle grazing incidence wide-angle scattering test method according to an embodiment of the present invention;

[0049] Figure 7 It is a diffraction angle 2Theta diagram (X-ray one-dimensional scattering diagram) obtained after scanning the integrated intensity according to the micro-area variable angle grazing incidence wide-angle scattering test method of an embodiment of the present invention;

[0050] Figure 8 Schematic diagram of an improved sample holder structure for a micro-area variable angle grazing incidence wide-angle scattering test method according to an embodiment of the present invention.

[0051] In the figure, 1. two-dimensional surface detector; 2. horizontal guide rail; 3. sample stage; 4. focusing mirror; 5. X-ray light source; 6. temperature control system; 7. imaging system; 8. collimator; 9. direct light blocker; 10. improved sample rack; 11. table; 12. height adjustment drive; 13. arc adjustment drive; 14. connection part; 15. X-axis adjustment screw; 16. Y-axis adjustment screw; 17. arc adjustment screw; 18. Z-axis height reference position; 19. arc track. DETAILED DESCRIPTION

[0052] Exemplary embodiments will be described in detail herein, examples of which are shown in the accompanying drawings. When the following description refers to the drawings, the same numbers in different drawings represent the same or similar elements unless otherwise indicated. The implementations described in the following exemplary embodiments do not represent all implementations consistent with one or more embodiments of this specification. Instead, they are merely examples of devices and methods consistent with some aspects of one or more embodiments of this specification as detailed in the appended claims.

[0053] It should be noted that: in other embodiments, the steps of the corresponding method are not necessarily performed in the order shown and described in this specification. In some other embodiments, the steps included in the method may be more or less than those described in this specification. In addition, a single step described in this specification may be decomposed into multiple steps for description in other embodiments; and multiple steps described in this specification may be combined into a single step for description in other embodiments.

[0054] Wide-angle scattering test methods and devices based on small-angle X-ray scattering instruments are commonly used materials analysis tools, and wide-angle scattering test methods based on single-crystal diffractometers have also been gradually developed and promoted. However, this device faces many problems in grazing-incidence wide-angle scattering tests.

[0055] Based on this, the present invention solves the problems existing in the prior art based on an improved sample holder.

[0056] Embodiment 1

[0057] The present invention aims to propose a micro-area variable angle grazing incidence wide-angle scattering test method, specifically, referring to Figure 1 , taking the PTO (PtTiO3, platinum titanate) thin film material deposited on the STO (SrTiO3, strontium titanate) substrate as an example, the following steps are included:

[0058] S00: Prepare a sample of the PTO thin film material deposited on the STO substrate and place it on the improved sample holder 10.

[0059] Among them, the single crystal diffractometer is an existing four-element diffractometer, which has four rotational degrees of freedom, namely vertical tilt, horizontal rotation, detector rotation and sample rotation. However, on this basis, the present invention designs digitally controlled tilt along the optical path direction, digital Z height precision control and feedback, and horizontal XY direction adjustment, that is, an improved sample holder 10, which directly replaces the original sample holder of the single crystal diffractometer with the improved sample holder 10, and is installed on the sample stage 3 of the single crystal diffractometer for installing the sample holder in the same installation method as the original sample holder (due to different structures of connecting the sample stage 3 of different single crystal diffractometers, the connection methods are all different. Taking the common structure as an example, a threaded connection structure is adopted).

[0060] Among them, single crystal diffractometers mainly include: Figure 2 As shown in the figure, there are two-dimensional surface detector 1, horizontal guide rail 2, improved sample holder 10, focusing mirror 4, X-ray light source 5 (also equipped with copper target or molybdenum target), temperature control system 6, imaging system 7, collimator 8, and direct light blocker 9. A two-dimensional surface detector 1 is slidably arranged on a horizontal guide rail 2, and can move away from or close to a sample stage 3 or make a horizontal circular rotation along the horizontal guide rail 2; the horizontal guide rail 2 is arranged at one end of the sample stage 3 away from a focusing mirror 4; an improved sample holder 10 is arranged on the sample stage 3; the focusing mirror 4 is connected to an X-ray light source 5 and is arranged at one end of the sample stage 3 away from the horizontal guide rail 2, and a collimator 8 arranged toward the sample stage 3 is arranged on the focusing mirror 4; a temperature control system 6 is arranged directly above the sample stage 3 and can move up and down to adjust the height, the tilt angle along the optical path direction, the tilt angle perpendicular to the optical path direction and the horizontal xy movement, and a direct light blocker 9 is arranged on the temperature control system 6; an imaging system 7 is arranged toward the improved sample holder 10, and the specific single crystal XRD structure is consistent with the authorized patent CN118243709B, the only difference is that the sample holder is different, and there is no external light source of the patent. Of course, it can also be combined with the external light source of the patent to further expand the single crystal-single crystal in-situ phase change atomic-level structure monitoring method.

[0061] Among them, the authorized patent CN118243709B cannot achieve variable angle grazing incidence wide angle scattering, and the introduction of this improved sample holder 10 solves the technical bottleneck of deep analysis of the atomic level structure of functional materials. It not only saves the cost of purchasing another X-ray wide angle scattering instrument, but also saves the cost of purchasing an in-situ cavity. The most important thing is that it expands the function of two-dimensional deep structure analysis of multi-field coupling driven by atmosphere + thermal energy, and successfully captures the process and mechanism of growth, aging or stability of two-dimensional photovoltaic materials and semiconductor materials, which has extraordinary scientific research significance and expands the breadth of characterization technology.

[0062] S10: Select an X-ray light source 5 so that the X-ray light source 5 is aimed at the sample, wherein the X-ray light source 5 is a switchable combination of a copper target and a molybdenum target.

[0063] S20: In the Z-scan scanning mode of the diffractometer, the X-ray light intensity is scanned in the vertical direction, and the film material with the substrate is adjusted to the test height by the lifting drive component; that is, the z coordinate is scanned from the lowest to the highest, and the light intensity is scanned from the highest intensity to the lowest intensity, and then the z height when the substrate material just covers half of the beamstop (direct light blocker 9) is taken, and the light intensity is about half of the direct light. The Z scanning range is 0-20mm, the step length is 0.1mm / step, and the scanning speed is 0.1s / step.

[0064] The lifting driving component is an additional structure of the single crystal diffractometer, which is used to drive the lifting of the sample stage 3.

[0065] like Figure 3 As shown in the figure, the scattering diagram obtained on the detector in the Z-scan scanning mode: the sample changes along the z-axis and reaches the center of the light blocker, which is the appropriate z-coordinate height. Figure 3 The alternation of light and dark is due to the fact that the substrate gradually blocks the direct light, leaving dark shadows.

[0066] S30: Perform tilt scanning (rocking) along the light path under the improved sample stage 3, scanning from the minimum light flux to the strongest light and then to the weakest light, and take the Theta angle when the light intensity is the strongest as the zero point of the light path direction. The rocking rotation axis is omega, and the direction is the horizontal plane of light travel. The rocking scanning range is -5-5°, the step length is 0.01° / step, and the scanning speed is 0.1s / step.

[0067] like Figure 4 As shown, the two-dimensional scattering diagram after the detector detects the signal.

[0068] S40: Set the distance between the sample and the detection surface of the single crystal diffractometer to 40-120 mm, set the exposure time to 1-300 s to collect the scattered signal, and set the incident angle to 0.1-10°.

[0069] like Figure 5 As shown in Figure 2, this is the two-dimensional scattering diagram of the detector after receiving the signal after the parameters are set.

[0070] S50: Collect the scattered X-rays through the two-dimensional surface detector 1. If the two-dimensional scattering image collected at this time shows that the substrate is tilted, another arc adjuster perpendicular to the optical path can be manually adjusted to place the substrate on a flat horizontal line to optimize the scattering intensity, such as Figure 5 and Figure 6 shown.

[0071] S60: The diffraction angle 2Theta diagram (one-dimensional X-ray scattering diagram) is obtained by integration through software (software package provided by the single crystal diffractometer); the incident angle is continuously changed, and the scattered X-rays are continuously collected through the two-dimensional surface detector, and a series of one-dimensional X-ray scattering diagrams are obtained through software integration, such as Figure 7 As shown in the figure (abscissa 2Theta, ordinate intensity), as the depth changes, X-rays penetrate from the shallow surface of the sample to the main body, carrying structural information at different depths. This is manifested as the appearance of new peaks, the disappearance of existing peaks, or changes in peak intensity and peak position drift.

[0072] In this embodiment, the sample holder 10 is improved as follows Figure 8As shown, the improved sample rack 10 is provided with a table 11 for placing the test material, a Z-axis height reference position 18, a height adjustment driver 12 (Z-axis height lifting motor) for driving the improved sample rack 10 to move back and forth along the Z-axis, an arc adjustment driver 13 (arc adjustment drive motor) for driving the improved sample rack 10 to make a curved swinging motion along the optical path direction, and a connection part 14 that cooperates with the sample stage 3 of the single crystal diffractometer, and the control of the incident angle is achieved through the arc adjustment driver 13. Specifically, the arc adjustment driver 13 drives the table 11 to slide back and forth on the arc track of the improved sample rack 10 through a lead screw transmission to achieve swing angle adjustment, and the swing angle is -15 ~ 15°, and the table 11 and the arc adjustment driver 13 are connected through an adapter bracket, that is, the arc adjustment driver 13 drives the adapter bracket to move horizontally, and then the table 11 and the adapter bracket are movably connected (such as hinged), so the bottom of the table 11 can slide back and forth on the arc track 19 of the improved sample rack 10 to achieve swing angle adjustment. Preferably, an arc adjustment screw 17 and an arc track 19 in another direction can be added to achieve the same operation. The two directions are perpendicular to each other. The arc adjustment screw 17 can also be installed with an arc adjustment driver 13 to slide back and forth on another arc track 19 of the improved sample holder 10 to adjust the swing angle, so as to achieve the flatness of the sample in the horizontal plane perpendicular to the light path direction, so that the sample can obtain a higher scattering intensity. Note: The two arc tracks 19 have the same function, only in different directions, so the same reference numerals are used.

[0073] The improved sample rack 10 is also provided with an XY two-axis adjustment structure - two adjustment screws (X-axis adjustment screw 15 and Y-axis adjustment screw 16), which also use the screw transmission principle to achieve horizontal adjustment of the improved sample rack 10. The height adjustment driver 12 converts the rotational motion into linear motion through a worm gear transmission method combined with a screw transmission method or other transmission methods, thereby achieving height adjustment of the table 11.

[0074] The driving mode of the motor here is preferably a worm gear combined with a screw drive (i.e., the principle of the existing turbine screw elevator. The various transmission modes in this scheme are common means in the mechanical field. The advantage is that it is integrated into a sample holder to achieve multi-degree-of-freedom adjustment, thereby expanding the test method of the existing XRD equipment). The sample holder has the following advantages:

[0075] 1. The improved sample holder 10 is flexible and compact, breaking through the limitation of the narrow space between the collimator and the light blocker, and can not only meet all the test requirements of micro-area variable angle grazing incidence scattering, but also maximize the protection of the safety of components such as detectors.

[0076] The space between the collimator and the light blocker is very limited and can only accommodate a 1cm x 1cm piece, so a small flat plate is supported by a thin rod on the sample holder to carry the 1cm x 1cm piece of sample. In this way, the sample will not touch any parts of the original diffractometer.

[0077] 2. We designed an incident angle that can accurately control the micro-region variable-angle grazing incidence scattering. Based on the original technology, we expanded the depth gradient analysis of thin film materials deposited on substrate materials and realized the structural gradient change from the surface to the body of the material, such as solar cell materials, organic photovoltaics, perovskite thin film samples, data storage and transmission chips, etc.

[0078] Due to the precise control of the motor along the light path direction, the improved sample holder 10 can perform high-precision curved rocking motion in the light path direction, thereby achieving precise control of the incident angle.

[0079] Digital high-precision height control uses a reference position as a standard reference point to ensure that the scattering spectra of all samples do not drift, that is, the standardization and reproducibility of the test peak position are ensured, thereby improving data quality (the reference position of the height, that is, when the sample stage 3 reaches the lowest position, the reference position value of the lowest position is 0 mm; the height based on this is accurate and has high reproducibility).

[0080] The Z-axis height is controlled by a lifting motor, so it can be digitally controlled with high precision. In addition, the newly designed sample stage 3 has a reference point, so the Z-axis height has a standard reference point as the zero point, which improves reproducibility and ensures high precision.

[0081] 4. High-precision micro-area analysis can be achieved: by fine-tuning x and y, micro-area variable-angle grazing incidence scattering characterization in different areas can be achieved. Figure 8 Adjust the front and rear position of the sample stage 3 by turning the screws in the middle.

[0082] 5. All motors in the present invention can be digitized and controlled by special external software.

[0083] Those skilled in the art should understand that the technical features of the above embodiments may be arbitrarily combined. To make the description concise, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0084] The above embodiments only express several implementation methods of the present invention, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the scope of the present invention. It should be pointed out that, for those of ordinary skill in the art, several modifications and improvements can be made without departing from the concept of the present invention, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the attached claims.

Claims

1. Micro-area variable angle grazing incidence wide-angle scattering test method, based on single crystal quaternary single crystal diffractometer, characterized in that: The following steps are involved: S00, preparing a sample of the test material deposited on the substrate and placing it on an improved sample holder; The improved sample holder is used to replace the original sample holder of the single crystal diffractometer, and the improved sample holder is provided with a table for placing test materials, a Z-axis height reference position, a height adjustment driver for driving the improved sample holder to move back and forth along the Z-axis, an arc adjustment driver for driving the improved sample holder to perform a curved swinging motion along the optical path direction, and a connection part that cooperates with the sample stage of the single crystal diffractometer, and the control of the incident angle is realized by the arc adjustment driver; S10, selecting an X-ray light source, aligning the X-ray light source at the sample, and switching between a copper target and a molybdenum target; S20, in the Z-scan scanning mode of the single crystal diffractometer, performing X-ray light intensity scanning in the vertical direction, and adjusting the test material with the substrate to a test height through the lifting drive component of the single crystal diffractometer; S30, performing a tilt scan along the optical path on the improved sample holder, scanning from the minimum light flux to the strongest light and then to the weakest light, taking the Theta angle when the light intensity is the strongest as the zero point of the optical path direction, and setting the distance between the sample and the detection surface of the single crystal diffractometer, the exposure time and the incident angle; S40, collecting scattered X-rays through a two-dimensional surface detector; S50, integrating by software of a single crystal diffractometer to obtain a one-dimensional X-ray scattering diagram; The incident angle is continuously changed, and the scattered X-rays are continuously collected through a two-dimensional surface detector, and then integrated through software to obtain a series of one-dimensional X-ray scattering maps.

2. The micro-area variable angle grazing incidence wide-angle scattering test method according to claim 1, characterized in that: The planar size of the table top of the improved sample rack is less than or equal to 1 cm x 1 cm.

3. The micro-area variable angle grazing incidence wide-angle scattering test method according to claim 1, characterized in that: In step S20, the scanning parameters of the Z-scan scanning mode are: Z scanning range 0-20 mm, step length 0.1 mm / step, and scanning speed 0.1 s / step.

4. The micro-area variable angle grazing incidence wide-angle scattering test method according to claim 1, characterized in that: In step S30, the distance between the sample and the detection surface of the single crystal diffractometer is 40-120 mm, the exposure time is 1-300 s, and the incident angle is 0.1-10°.

5. The micro-area variable angle grazing incidence wide-angle scattering test method according to claim 1, characterized in that: The Z-axis height reference position is 0mm.

6. The micro-area variable angle grazing incidence wide-angle scattering test method according to claim 1, characterized in that: The improved sample rack is also provided with an adjustment structure for adjusting the horizontal position of the table top.

7. The micro-area variable angle grazing incidence wide-angle scattering test method according to claim 6, characterized in that: The adjustment structure includes an X-axis adjustment screw for adjusting the X-axis position of the table and a Y-axis adjustment screw for adjusting the Y-axis position of the table.

8. The micro-area variable angle grazing incidence wide-angle scattering test method according to any one of claims 1 to 7, characterized in that: The connecting part is screwed to install the improved sample holder on the sample stage base of the single crystal diffractometer.

9. The micro-area variable angle grazing incidence wide-angle scattering test method according to any one of claims 1 to 7, characterized in that: The sample rack is also provided with an arc adjustment screw for the tabletop swing arc, which is arranged perpendicularly to the output shaft of the arc adjustment driver and can adjust the substrate to a flat horizontal line to optimize the scattering intensity.

10. The micro-area variable angle grazing incidence wide-angle scattering test method according to claim 9, characterized in that: The arc adjustment screw rod is also connected with an arc adjustment driver.

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